反应详情

A suspension of 3.28 g (9.1 mMol) of {4-[4-(6-methoxy-pyridin-3-ylmethylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-phenyl}-methanol in 40 ml of acetonitrile, 40 ml of dioxane and 4 ml of SOCl2 is stirred for 1 h at RT. The mixture is dissolved in EtOAc and NaHCO3-solution, the aqueous layer separated off and extracted with EtOAc. The organic layers are washed with NaHCO3-solution, water and brine, dried (Na2SO4) and partially concentrated. The crystallized title compound can be filtered off; elemental analysis for C, H and N within 0.4% of calculated value.

1. customNaHCO3-solution, the aqueous layer separated off
2. extractionextracted with EtOAc
3. washThe organic layers are washed with NaHCO3-solution, water and brine
4. dry with materialdried (Na2SO4)
5. concentrationpartially concentrated
6. customThe crystallized title compound
7. filtrationcan be filtered off